A novel experimental approach for nanostructure analysis: simultaneous small-angle X-ray and neutron scattering

Abstract

Exploiting small-angle X-ray and neutron scattering (SAXS/SANS) on the same sample volume at the same time provides complementary nanoscale structural information in two different contrast situations. Unlike an independent experimental approach, the truly combined SAXS/SANS experimental approach ensures the exactness of the probed samples, particularly for in situ studies. Here, an advanced portable SAXS system that is dimensionally suitable for installation in the D22 zone of ILL is introduced. The SAXS apparatus is based on a Rigaku switchable copper/molybdenum microfocus rotating-anode X-ray generator and a DECTRIS detector with a changeable sample-to-detector distance of up to 1.6 m in a vacuum chamber. A case study is presented to demonstrate the uniqueness of the newly established method. Temporal structural rearrangements of both the organic stabilizing agent and organically capped gold colloidal particles during gold nanoparticle growth are simultaneously probed, enabling the immediate acquisition of correlated structural information. The new nano-analytical method will open the way for real-time investigations of a wide range of innovative nanomaterials and will enable comprehensive in situ studies on biological systems. The potential development of a fully automated SAXS/SANS system with a common control environment and additional sample environments, permitting a continual and efficient operation of the system by ILL users, is also introduced. research papers J. Appl. Cryst. (2020). 53, 722-733 Ezzeldin Metwalli et al. Simultaneous SAXS/SANS 723

Soft Matter Sample Environments for Time-Resolved Small Angle Neutron Scattering Experiments: A Review

“…Until recently, such a combination was not feasible, but developments in X-ray generation and detector technology have allowed the first steps in allowing such a combined scattering instrument to be developed. Specifically, the two probe beams were placed at right angles to one another, making the system less useful for samples that are anisotropic, but it can serve as a proof of principle [155]. The complication that one faces with the development of such an instrument is that one invariably tries to mount an X-ray system on an existing neutron scattering beamline.…”

The Importance of Interphases in Energy Storage Devices: Methods and Strategies to Investigate and Control Interfacial Processes

“…Indeed, neutron reflectometry offers the possibility to obtain quantitative information on the Li concentration in the amorphous SEI layer. Neutrons are also exploited for the small angle neutron scattering (SANS) and inelastic neutron scattering (INS) techniques, providing information about the size, shape, volume of nanostructures of the interphase layers in the range of 5-200 nm [59][60][61][62][63][64].…”

Simultaneous SAXS/SANS Method at D22 of ILL: Instrument Upgrade

“…A key contribution of the simultaneous SAXS/SANS method is its ability to perform in situ and operando studies on advanced materials that undergo temporal modifications under external stimuli [23], allowing access to their structural rearrangements from the molecular scale to nanoscale assemblies. This means not only the synergy that results when data sets are obtained simultaneously from the same sample volume, but also access to the cross-correlation of phases/components when two different simultaneous contrast situations are probed for multi-phase/component samples.…”

“…This means not only the synergy that results when data sets are obtained simultaneously from the same sample volume, but also access to the cross-correlation of phases/components when two different simultaneous contrast situations are probed for multi-phase/component samples. For instance, the cross-correlation between evolved gold nanorods size/shape (SAXS) and the corresponding engaged structure of organic moieties (SANS) during surfactant-assisted seed-mediated synthesis of gold nanorods will reveal new information related to the exact growth mechanisms involved [23]. Moreover, the SAXS/SANS system will enable contrast-dependent successive length-scale characterization of novel nanomaterials, addressing unsolved scientific questions.…”